Esterification of oils



Jan. 22', 1924.

E. R. BOLTON ET- AL ESTERIFICATION OF OILS Filed Fe b. 21 1921 Irwenlbrs E. 15. fiallon- E. J Law];

ozli'ornlf 1e pared.

Patented Jan. 22, 1924.

warren stares tasters sates;

EWARJD RICHARDS BOLTON AND ERNEST JOSEPH LUSH, OF LONDON, ENGLAND, AS-

SIGNORS TO TECHNICAL RESEARCH WORKS, LIMITED, OF LONDON; ENGLAND.

ES TERIFIQATION OF OILS.

' Application filed'February 21, 1921. Serial 446,868.

plication in England September 30, 1919,

application No. 23,957), of which the followmg is a specification.

It is well known that the fatty acids such as oleic acid combine, with glycerine'with" the production of glycerides, in which manner mono-- ditriglycerides have been pre- For, example oleic acid and palmitic acid have already been converted into olein and palmitin b heating such acids with a quantity of .g ycerine, while employing considerable time for eflecting the des'.'ed neutralization .(esterification) this reaction being somewhat slow, on account of-the ac cumulation of water'in the mixture and the; immiscibility of the two liquids.

The present invention, relatesto an improved process forproducing glycerides characterized by the fact that: such glyc+ erides are produced in a comparatively short time and very economically, whereby the deso sired qualities of colour, taste and smell are assured in a more efficient manner than heretofore.

The method of procedure according to the present invention is as follows j so The free fatty acids or the oil or fat containing free fatty acids as may be desired containedin a suitable receptacle, ac

cording to the useto be made of the finished product, are subjected to the action of glycco erine vapours whereby chemical action takes place between the fatty acids and the glycerine' vapours, resulting in the productlon of glycerides and water, which latter comes off as steam and must be'removed, and any ee glycerine thus carried over may be recovered. The glycerine vapours are passed into the fatty acids or oil or fat containing free fatty acids, and the glyoerine and oil may be in separate vessels. The admissionand so distribution of the glycerine vapour throughout the body of the fatty acids to be treated can be carried out in a variety of ways for example by the employment of a perforated coil of piping situated at or near the botcc tom of the vessel.

Or the glycerine may be vaporized by the oil or fat containing free fatty acids contained in the vessel, the contents of which are heated to a temperature above the boiling point of glycerine so that when the .lat-

ter is introduced at or near the bottom, the vapour generated will rise through the oil contents and act on the free fatty acids producing glycerides. With this method of carrying out theprocess an addition of a small amount, say two per cent, of water to the glycerine will facilitate the produc-' tion of the glycerine vapours,and dispense with the employment of superheated steam as is preferably used when the glycerine is vaporized in a separate vessel.

In connection. with this process the use of vacuum is desirable as a much lower temperature is required for the distillation ofglycerine, in consequence'of which the percentage of decomposition of glycerine is reduced to a minimum.

In the annexed-drawing is diagrammatically illustrated by way of example, a simple form of apparatus suitable for carrying out the process as first referred to in the above description'in whichthe vessel a rep resents the glycerine still and the vessel 6 the receptacle for the oil tobe subjected to the-treatment. Both the vessels 1- and b are hermetically sealed by any convenient means and are provided withzheati'ng c'riils i c and d that are supplied with superheated steam from the main supply 6 regulated b the valvesf and g. Live steam which is also preferably superheated is admitted to the vessels'aand b by the supply i-pes h' and z through the depending pipes y and'k that may have aflixed to their lower ends any form of distributor. The vessels a and b i are connected together by means of the pipe m so that they are both subjected to the action of a vacuum pump, witha condenser and receiver interposed between the'vacuum pump and thevessel 72, communication being' established by the outlet pipe. at 'forthe purpose of obtainin the necessary vacuum in the vessels (1 am? valves 0 and ;0 being interposed in the pipes It and m therefor.

It will now be understoodthat the vaporized glycerine which may be obtained from crude glycerine placed'in the vessel} a is carried over into the vessel 5 by the pipe m and is discharged at or near to the 6, suitable non-return.

i v 1 Jim I bottom-pf the to' mix in' a;

with the oil in the-said l. b which .0 is maintained at a tem rature from at least j 160.to 250 centigra e.b";t he, heatingrcoil d. The vaporizationofit e'gl cerine is fa-' in the veael cilita ted by the vacuum form 1 a, andisv-efi'ected h the steam supply to the heating coil 0, 0' course assisted by the steam introduced through pipe 7'. Hence the process consists in the esterification of the oil coxitaiiiedin the vesselb'b passing H 'therethrough g1 eerinefvapour ormed 'in rpm-1 sea or or di ierpu the vessel a, e. process .canbe readily carried out so that no'fexcess of glycerine' is present in theoil treated thus avoiding the necessity of recovery thereof and by the aforesaid method much time is saved in obtaining the desiredefiact; for from experiments made we have found that it isp'ossibleto treat oil containingv 50 per cent of free fatty acids satisfactorilywithin the period of onehoim- This invention is the treatment of oils where the presence. of free fattyiacids is objectionable, for" example, as an operation preliminary to the .hydrogenation of oilsfinf processes where a neutral oil is requiredyor in such refining 3 recesses where considerable loss is incur-re ue to free fatty acids as for example in the refining ofoilsqwith-an alkali for edible high grade 'soa sand the like rpo'se's for whic o glycerin'e vapour in the manner described .the e production of diand mono-glycerides 1s readily obtained anjd'in orderto hasten the reaction any known form of catal may be emplplyed but generally '8 such we have foun sor unnecessary. v

at we claim is 19- 1.. .A process of treating fatty comprises heating an oil cents anaddition or. acees-.

oils which an undesirably large excess of free'fatty acid, to

least, of the free fatt especially applicable refined; B combinatlon-withthe requisite amount a temperature of between 160 and 250 0., and whilesuch oil is-at said temperature introducin thereinto, acurrentof va r o glycerin mixed with steam,- and continuing such mixture of vapors,

therefrom at least'of the free fatty-acid present has been converted into glicerids 'of fatty acids."

The process for t acids or' oils or fats containin free fatty acids-into lycerides which consists-m heating such su stances preparatory to and dur-' mg such conversion to a temperature of at. least 160 centigiade but not exceeding 250,

centigrade and subjecting the same to the action of glycerine vapour generated by superheated steam under vacuum.

. 4. The process for the conversion of fatty acids oroi'ls'or fats containi fatty acids into glyc'erides which consists in heating such substances preparatory'to and during such conversion to a temperature of at least 160 'centigrade but not exceeding-250 catal st, sai ated y superheated steam under vacuum.

. In testimony whereof we have ournames to this specification.

EDWARD mans .BOLTONgE- ERNEST JOSEPH LUSH, c

e conversion of fatty centigrade and subjecting the same to theaction of glycerine vapour with a suitable glycerine vapour b'eing gener-Q 

